STANDARD OPERATING PROCEDURE

Title: VOLUMETRIC SOLUTIONS DEPARTMENT: QC

SOP NO.: QC-07 Supersede No.: New
Effective Date: April 26, 2011 Page: 1 of 12

OBJECTIVE:
To provide a guideline for the standardization of volumetric solutions.

SCOPE:
Applicable to the volumetric solutions used for chemical analysis.

RESPONSIBILITY:
Analyst & Q.C. Incharge.

PROCEDURE :
Volumetric solutions are standardized by titration against a primary standard or a standard solution,
previously standardized against a primary standard.

Primary standard must be obtainable in very pure state reasonably high formula weight, readily
soluble in the solvent to be used, sufficiently stable and unchanged in atmospheric air.

Standard solutions are prepared by accurately weighing a quantity of primary standard equivalent
to gram equivalent weight per liter(for normal solution) and gram molecular weight per liter (for
molar solution), and do not require standardization initially.

Volumetric solutions are standardized following the procedure mentioned in this SOP and the
normality factor is calculated up to third decimal assigning the usage life depending upon stability.

Calculations will be recorded in a note book along with index content and reviewed by
Q.C.Incharge.

Volumetric Solutions that are not used frequently or whose strength changes will be standardized
on the day of use.

Volumetric solutions prepared by exact dilution of a stronger standardized solution do not require
standardization initially and thus the same normality factor will be used.

Volumetric solutions that show evidence of sedimentation or crystallization will be discarded

regardless of age.
 STANDARD OPERATING PROCEDURE
Title: VOLUMETRIC SOLUTIONS DEPARTMENT: QC
SOP NO.: QC-07 Supersede No.: New
Effective Date: April 26, 2011 Page: 2 of 12

Volumetric solutions are kept in amber glass bottles properly labeled indicating the name, strength,
usage life, prepared on and prepared by etc.

Ready to use or highly stable volumetric solutions will be re-standardized at regular interval to
confirm the usage status throughout the shelf life.

Standardization procedures of volumetric solutions are given on Annexure I, against their

individual titles.

Shelf life of the volumetric solutions is given on Annexure II.

Standardization record for each volumetric solution will be retained for 1 year after the solution
was exhausted.

HISTORY : NEW
 STANDARD OPERATING PROCEDURE
Title: VOLUMETRIC SOLUTIONS DEPARTMENT: QC
SOP NO.: QC-07 Supersede No.: New
Effective Date: April 26, 2011 Page: 3 of 12
Annexure I
STANDARDIZATION PROCEDURE
NOTE: The following methods have been derived from United States Pharmacopeia .

(01) Ammonium thiocyanate, Tenth-Normal (0.1N)

NH4SCN, 76.12
7.612g in 1000ml
Dissolve 8g of ammonium thiocyanate in 1000ml of water, and standardize the solution as follows.
Accurately measure about 20ml of 0.1N silver nitrate VS into a glass-stopper flask. Dilute with
50ml of water, then add 10ml of 5N nitric acid and 2ml of ferric ammonium sulfate TS, and titrate with the
ammonium thiocyanate solution to the first appearance of a red-brown color.

N.F. = ml of AgNO3 × N AgNO3

ml NH4SCN Solution
N.F. = Normality factor.
If desirable, 0.1N ammonium thiocyanate may be replaced by 0.1N potassium thiocyanate where the
former is directed in various tests and assays.

(02) Bromine, Tenth-Normal(0.1 N)

Br, 79.90
7.990 g in 1000ml

Dissolve 3 g of potassium bromate and 15 g of potassium bromide in water to make 1000 ml, and
standardize the solution as follows.
Accurately measure about 25 ml of the solution into 500ml iodine flask and dilute with 120ml
of water. Add 10ml of 5N hydrochloric acid, insert the stopper in the flask ,and shake it gently then add
5ml of potassium iodide TS, again insert the stopper, shake the mixture, allow it to stand for 5 minute, and
titrate the librated iodine with 0.1N sodium thiosulphate VS, adding 3ml of starch TS as the endpoint is
approached & continuing the titration to the first appearance of colorless solution.

N.F. = ml Na2S2O3 × NNa2S2O3

ml Br2 solution
 STANDARD OPERATING PROCEDURE
Title: VOLUMETRIC SOLUTIONS DEPARTMENT: QC
SOP NO.: QC-07 Supersede No.: New
Effective Date: April 26, 2011 Page: 4 of 12

(03) Ceric Ammonium Nitrate, Tenth -Normal(0.1N)

Ce(NO3)4.2NH4NO3, 548.22
5.482 g in 100 ml

Dissolve 5.5 g of ceric ammonium nitrate in 1 N nitric acid to obtain 100 ml of solution. Filter (if
necessary) and then Standardize the solution as follows.
Accurately measure 10 ml of freshly standardized 0.1 N ferrous ammonium sulfate VS into a
flask, and dilute with water to about 100 ml. Add 2 drop of nitrophenanthroline TS , and titrate with the
ceric ammonium nitrate solution to a colorless endpoint.

N.F. = ml Fe(NH4)2(SO4)2 × N Fe(NH4)2(SO4)2

ml Ce(NO3)4 . 2NH4NO3

(04) Edetate Disodium , Twentieth-Molar ( 0.05 M )

C10H14N2Na2O8.2H2O , 372.24
18.61 g in 1000 ml
Dissolve 18.7 g of edetate disodium in water to make 1000 ml, and standardize the solution as follows.
Accurately weigh about 200 mg of chelometric standard calcium carbonate, previously dried at 110° for 2
hrs and cooled in a desiccator, transfer to a 400 ml beaker, add 10 ml of water and swirl to form slurry.
Cover the beaker with a watch glass, and introduce 2 ml of diluted hydrochloric acid from a pipette inserted
between the lip of the beaker and the edge of the watch glass. Swirl the contents of the beaker to dissolve
the calcium carbonate. Wash down the sides of the beaker, and the outer surface of the pipette, and the
watch glass with water, and dilute with water to about 100 ml. While stirring the solution, preferably with a
magnetic stirrer, add about 30 ml of 0.05M Edetate disodium from a 50 ml burette. Add 15 ml of sodium
hydroxide TS and 300 mg of hydroxyl naphthol blue, and continue the titration with 0.05M Edetate
disodium to a blue endpoint. Each 5.005 mg of CaCO3 is equivalent to 1 ml of 0.05M EDTA.

M.F. = Morality factor M.F. = mg CaCO3__

5.005 × ml EDTA
 STANDARD OPERATING PROCEDURE
Title: VOLUMETRIC SOLUTIONS DEPARTMENT: QC
SOP NO.: QC-07 Supersede No.: New
Effective Date: April 26, 2011 Page: 5 of 12

(05) Ferrous Ammonium Sulfate, Tenth Normal (0.1 N)

Fe(NH4)2(SO4)2 .6H2O , 392.14
39.21 g in 1000ml
Dissolve 40 g of ferrous ammonium sulfate in a previously cooled mixture of 400ml of sulfuric acid and
200 ml of water, dilute with water to 1000ml, and mix. On the day of use, standardize the solution as
follows.
Accurately measure 25 ml of the solution into a flask, add 2 drops of nitrophenanthroline TS; and
titrate with 0.1 N ceric ammonium nitrate VS to a colorless endpoint.

N.F. = ml Ce(NO3)4.2NH4NO3 × N Ce(NO3)4.2NH4NO3

ml Fe(NH4)2(SO4)2

(06) Hydrochloric Acid , Tenth-Normal (0.1 N )

HCl , 36.46
3.646 g in 1000 ml

Dilute 8.5 ml of hydrochloric acid with water to 1000 ml .Standardize the solution as follows.
Accurately weigh about 300mg of tromethamine, previously dried at 105° for 3 hours. Dissolve
in 50 ml of water, and add 2 drops of bromocresol green TS. Titrate with 0.1N hydrochloric acid to a pale
yellow end point. Each 12.114 mg of tromethamine is equivalent to 1 ml of 0.1N hydrochloric acid.

N.F. = mg tromethamine
12.114 × ml HCl
 STANDARD OPERATING PROCEDURE
Title: VOLUMETRIC SOLUTIONS DEPARTMENT: QC
SOP NO.: QC-07 Supersede No.: New
Effective Date: April 26, 2011 Page: 6 of 12

(07) Iodine, Tenth-Normal (0.1 N)

I, 126.90
12.69 g in 1000 ml
Dissolve about 13 g of iodine in a solution of 36 g of potassium iodide in 100 ml of water, add 3 drops of
hydrochloric acid, dilute with water to 1000 ml, and standardize the solution as follows.
Transfer 20 ml of the iodine solution to a 500 ml stoppered flask, add 5 ml of 5 N hydrochloric acid,
swirl gently to mix, and titrate with 0.1 N sodium thiosulfate VS until the solution has a pale yellow color.
Add 2 ml of starch TS and continue titrating until the solution is colorless.

N.F. = ml Na2S2O3 × N Na2S2O3

ml I2

(08) Perchloric Acid, Tenth-Normal (0.1 N) in Glacial Acetic Acid

HClO4, 100.46
10.05 g in 1000 ml
(Ready-to-use solution)
Accurately weigh about 200 mg of potassium biphthalate, previously dried at 120°C for 2 hrs, and dissolve
in 50 ml of glacial acetic acid in a 250 ml dry stoppered flask (heat if required). Add 1 small crystal of
crystal violet, and titrate with the Perchloric acid solution until the color changes to blue-green. Deduct the
volume of the Perchloric acid consumed by 50 ml of the glacial acetic acid (blank). Each 20.42 mg of
potassium biphthalate is equivalent to 1 ml of 0.1 N Perchloric acids.

N.F. = mg KHC8H4O4 .
20.42 × ml HCl4
 STANDARD OPERATING PROCEDURE
Title: VOLUMETRIC SOLUTIONS DEPARTMENT: QC
SOP NO.: QC-07 Supersede No.: New
Effective Date: April 26, 2011 Page: 7 of 12

(09) Potassium dichromate, Tenth –normal (0.1N)

K2Cr2O7, 294.18
4.903 g in 1000 ml

Dissolve about 5 g of potassium dichromate in 1000 ml of water. Standardize the solution as follows.
Transfer 20 ml of this solution to a 500-ml glass–stoppered flask, add 2g of potassium iodide, add 5 ml of
5N hydrochloric acid, allow to stand for 10 minutes in a dark place, and titrate the liberated iodine with
0.1N sodium thiosulfate VS adding 3 ml of starch TS as the endpoint is approached; continue titration until
a green color is obtained.

N.F. = ml Na2S2O3 x N Na2S2O3

ml K2Cr2O7

(10) Potassium hydroxide, Alcoholic, Half-Normal (0.5 N)

28.06 g in 1000 ml

Dissolve about 30 g of potassium hydroxide in 50 ml of water and add methyl alcohol to make 1000 ml .
Allow the solution to stand in a tightly-stoppered bottle for 24 hours. Then decant the clear supernatant into
a tightly stoppered bottle and standardize the solution as follows. Accurately measure about 50 ml of 0.1N
hydrochloric acid VS, add 2 drops of phenolphthalein TS, and titrate with the alcoholic potassium
hydroxide solution until a permanent pink color is produced.
N.F. = ml HCl x N HCl
ml KOH
 STANDARD OPERATING PROCEDURE
Title: VOLUMETRIC SOLUTIONS DEPARTMENT: QC
SOP NO.: QC-07 Supersede No.: New
Effective Date: April 26, 2011 Page: 8 of 12

(11) Silver Nitrate, Tenth – Normal (0.1N)

Ag NO3 169.87
16.99 g in 1000 ml

Dissolve 17 g of silver nitrate in 1000 of water, and standardize the solution as follows.
Transfer 200mg, accurately weighed, potassium chloride, previously dried at 110°C for 2
hours to a 500ml conical flask. Dissolve in 25 ml of water and add 10 ml of glacial acetic acid, 50 ml of
methanol and about 2 drops of eosin-Y TS and mix. Titrate with the silver nitrate solution until an orange
pink color is obtained at the endpoint. Each 7.455 mg of potassium chloride is equivalent to 1 ml of 0.1N
silver nitrate.

N.F. = ______mg_KCl______
ml AgNO3 x 7.455

(12) Sodium Hydroxide, Tenth-Normal (0.1 N)

NaOH, 40.00
4.0 g in 1000 ml

Dissolve 4.2 g of sodium hydroxide in 1000ml of freshly boiled and cooled water. Accurately weigh
200mg of potassium biphthalate, previously dried at 120°C for 2 hours, and dissolve in 50 ml of water.
Add 2 drops of phenolphthalein TS, and titrate with the sodium hydroxide solution to the production of a
permanent pink colour. Each 20.42 mg of potassium biphthalate is equivalent to 1 ml of 0.1N sodium
hydroxide.

N.F. = mg KHC8H4O4 .
20.42 × ml NaOH
 STANDARD OPERATING PROCEDURE
Title: VOLUMETRIC SOLUTIONS DEPARTMENT: QC
SOP NO.: QC-07 Supersede No.: New
Effective Date: April 26, 2011 Page: 9 of 12

(13) Sodium nitrite, Tenth–molar (0.1 M)

NaNO2 68.00
6.900 g in 1000 ml

Dissolve 7 g of sodium nitrite in water to make 1000 ml, and standardize the solution as fallows.
Accurately weigh about 200 mg of sulfanilamide, previously dried at 105° for 3 hours, and transfer into a
500ml conical flask. Add 20 ml of hydrochloric acid and 50 ml of water sonicate until dissolved. Cool to
15°C and titrate with the standard solution maintaining the temperature at about. 15°C potentiometrically.
Each 17.22 mg of sulfanilamide is equivalent to 1 ml of 0.1M sodium nitrite.

M.F. = mg of sulfanilamide
17.22 x ml NaNO2
(14) Sodium thiosulfate, Tenth-Normal (0.1 N)
Na 2S2O3. 5H2O, 248.19
24.82g in 1000 ml

Dissolve 25 g of sodium thiosulfate and 200 mg of sodium carbonate in 1000ml of water and standardize
the solution as follows.
Accurately weigh 200 mg of potassium dichromate, previously dried at 130 °C for 2
hours .Dissolve in 50 ml of water by sonication .Add 3 g of potassium iodide, 2 g of sodium bicarbonate,
and 5ml of hydrochloric acid. Stand in the dark for 10 minutes and titrate the liberated iodine with the
sodium thiosulfate solution until the solution is yellowish green in color. Add 3ml of starch TS and
continue the titration until the blue color is discharged. Each 4.903 mg of potassium dichromate is
equivalent to 1 ml of 0.1N sodium thiosulfate.

N.F. = mg K2Cr2O7____
4.903 x ml Na2S2O3
 STANDARD OPERATING PROCEDURE
Title: VOLUMETRIC SOLUTIONS DEPARTMENT: QC
SOP NO.: QC-07 Supersede No.: New
Effective Date: April 26, 2011 Page: 10 of 12

(15) Sulfuric Acid , Tenth-Normal (0.1 N )

H2SO4 , 98.08
4.904 g in 1000 ml

Dilute 2.8 ml of sulfuric acid with water to 1000 ml .Standardize the solution as follows.
Accurately weigh about 0.3 g of tromethamine, previously dried at 105° for 3 hours. Dissolve
in 50 ml of water, and add 2 drops of bromocresol green TS. Titrate with 0.1N sulfuric acid to a pale
yellow end point. Each 12.114 mg of tromethamine is equivalent to 1 ml of 0.1N sulfuric acid.

N.F. = mg tromethamine
12.114 × ml H2SO4

(16) Tetrabutylammonium hydroxide in methanol Tenth-Normal (0.1N)

(C4H9)4NOH, 259.47
25.95 g in 1000 ml
(Ready-to-use solution)

Accurately weigh 100 mg of benzoic acid, previously dried at 105°C for 2 hrs, and dissolve in 50 ml of
dimethylformamide in a 500 ml stoppered flask. Add 3 drops of thymol blue TS (in dimethylformamide)
and titrate with TBAH solution until the color changes to blue at the endpoint. Deduct the volume of
TBAH solution consumed by 50 ml of dimethylformamide (blank). Each 12.21 mg of benzoic acid is
equivalent to 1 ml of 0.1 N TBAH.

N.F. = mg benzoic acid

12.21 x ml TBAH
 STANDARD OPERATING PROCEDURE
Title: VOLUMETRIC SOLUTIONS DEPARTMENT: QC
SOP NO.: QC-07 Supersede No.: New
Effective Date: April 26, 2011 Page: 11 of 12

(17) Zinc Sulfate, Twentieth-Molar (0.05 M)

ZnSO4. 7H2O, 287.56
14.4 g in 1000 ml

Dissolve 14.4 g of zinc sulfate in water to make 1000 ml. Standardize the solution as follows. Accurately
measure 20 ml of 0.05 M edetate disodium VS into a 500-ml conical flask, and add, in the order given, 20
ml of acetic acid-ammonium acetate buffer TS(USP 2005 page 2855), 50ml of; methanol, and 2 ml of
dithizone TS. Titrate with the zinc sulfate solution to rose-pink color at the endpoint.

M.F. = ml edetate disodium × Meditate disodium

ml ZnSO4
 STANDARD OPERATING PROCEDURE
Title: VOLUMETRIC SOLUTIONS DEPARTMENT: QC
SOP NO.: QC-07 Supersede No.: New
Effective Date: April 26, 2011 Page: 12 of 12

ANNEXURE
LIST OF VOLUMETRIC SOLUTIONS

SL. NO. NAME SHELF LIFE

1 Ammonium thiocyanate, Tenth-Normal (0.1N) 4 Months

2 Ammonium ferrous sulphate, Tenth-Normal (0.1N) 4 Months

3 Bromine, Tenth-Normal(0.1 N) 6 Months

4 Ceric ammonium nitrate, Tenth -Normal(0.1N) 6 Months

5 Edetate disodium , Twentieth-Molar ( 0.05 M ) 6 Months

6 Hydrochloric acid , Tenth-Normal (0.1 N ) 6 Months

7 Iodine, Tenth-Normal (0.1 N) 6 Months

8 Perchloric acid in Glacial acetic acid, Tenth-Normal (0.1 N) Ready to use 6 Months
(revalidate)
9 Potassium dichromate, Tenth –Normal (0.1N) 6 Months

10 Potassium hydroxide, Alcoholic, Half-Normal (0.5 N) 4 Months

11 Silver nitrate, Tenth – Normal (0.1N) 4 Months

12 Sodium hydroxide, Tenth Normal (0.1N) 4 Months

13 Sodium thiosulfate, Tenth-Normal (0.1N) 4 Months

14 Sodium nitrite, Tenth-Normal (0.1N) 4 Months

15 Sulfuric Acid , Tenth-Normal (0.1N) 6 Months

16 Tetrabutylammonium hydroxide in methanol, Tenth-Normal (0.1N) Ready to use 6 Months

(revalidate
17 Zinc Sulfate, Twentieth-Molar (0.05M) 6 Months
 STANDARD OPERATING PROCEDURE

DEPARTMENT: QC SOP NO.: QC-07

Effective Date: April 26, 2011 Supersede No.: New

TITLE: VOLUMETRIC SOLUTION

Total no. of pages: 13 (including covering page) Revision: After 3 Yrs.

Prepared by: Checked by: Approved by:

(Sr. Analyst) (Q.C. Manager) (Q.A. Manager)